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A kind of synthetic method of ammonium dihydrogen phosphate compound

A technology of ammonium dihydrogen phosphate and synthesis method, applied in the directions of phosphate, phosphorus oxyacid, electrical components, etc., can solve the problems of uneven dispersion, low temperature of grinding slurry, uneven carbon coating, etc. Uniform distribution and stable carbon content

Active Publication Date: 2016-04-06
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the electrochemical performance of carbon-coated modified lithium iron phosphate materials, the preferred carbon source is organic sugars, especially sucrose and glucose, but when using ferrous oxalate as the iron source, organic solvents (especially absolute ethanol and acetone) In the process route of synthesizing lithium iron phosphate in the system, there is uneven carbon coating caused by the uneven mixing of the added carbon source. Uneven dispersion. At the same time, because the grinding equipment uses low-temperature cooling water to reduce a large amount of heat energy generated during the grinding process, the temperature of the grinding slurry is lower, which makes the sugars not suitable for dissolution and dispersion, and finally leads to the appearance of uneven carbon coating.
Carbon coating is one of the commonly used methods in the modification of lithium iron phosphate, but due to the carbon addition method and uneven coating, the synthesized lithium iron phosphate is unstable in batches in terms of carbon content, which affects the processing of materials performance

Method used

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Examples

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preparation example Construction

[0013] The synthetic method of ammonium dihydrogen phosphate complex comprises the following method steps:

[0014] (1) Dissolve ammonium dihydrogen phosphate with deionized water, configure it as a supersaturated solution at a temperature of 20-100°C, and dissolve organic sugars with deionized water. The organic sugars are sucrose, glucose, fructose, and maltose One or more than two kinds are configured at this temperature to form an organic sugar solution with a mass fraction of 30-80%. Under stirring, mix the above two solutions evenly, and let stand for use;

[0015] (2) Add the mixed solution to the organic solvent at a speed of 5-1000 mL / min under stirring. The organic solvent is one or both of absolute ethanol and acetone at normal temperature. After completion, stand still at room temperature for 1-5 hours, filter to obtain the crystalline product, and dry the obtained crystalline product at low temperature to prepare the ammonium dihydrogen phosphate complex. The lo...

Embodiment 1

[0017] Take 500g of commercially available industrial grade ammonium dihydrogen phosphate, dissolve it with deionized water at 25°C to form a supersaturated solution, take 65g of sucrose and dissolve it with deionized water to form a sucrose solution with a mass fraction of 40%, and mix the above The two solutions were mixed, and the mixed solution was peristaltly added to absolute ethanol at a speed of 500mL / min. In the actual production process, the agitator was turned on, and after the addition was completed, it was left to stand at room temperature for 1 hour, and the crystals were precipitated by filtration, and the solid was separated from the solution. The filtered product was dried at 0°C for 2 h before use.

[0018] Application of ammonium dihydrogen phosphate compound: Weigh battery-grade lithium carbonate, battery-grade ferrous oxalate and synthesized ammonium dihydrogen phosphate compound according to the Li:Fe:P molar ratio of 1.01:1:1.05. Grind for 2 hours in an ...

Embodiment 2

[0020] Take 500g of commercially available industrial grade ammonium dihydrogen phosphate, dissolve it with deionized water to form a supersaturated solution at 40°C, take 68g of glucose to form a 50% glucose aqueous solution by mass fraction, mix the two solutions under constant stirring, and mix the mixed solution Add to acetone at a rate of 200mL / min, turn on the stirrer during the addition, and stand still at room temperature for 2 hours after the addition is completed. The crystals are precipitated by filtration, and the solid is separated from the solution. The filtered product is dried at -5°C for 4 hours before use.

[0021] Application of ammonium dihydrogen phosphate compound: Weigh battery-grade lithium carbonate, battery-grade ferrous oxalate and synthesized composite ammonium dihydrogen phosphate respectively according to the Li:Fe:P molar ratio of 1.01:1:1.04. Grind for 2 hours in an anhydrous ethanol system in a stirring grinder. After grinding, the slurry is dyn...

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Abstract

The invention discloses a method for synthesizing an ammonium dihydrogen phosphate compound. The method comprises the following steps: dissolving ammonium dihydrogen phosphate in deionized water, preparing a super-saturated solution at a certain temperature, dissolving organic sugar in deionized water, preparing an organic sugar solution with a certain mass percent at the temperature, uniformly mixing the two solutions in a stirring state, and standing for later use; and adding the mixed solution into an organic solvent in a stirring state according to a certain speed, standing at room temperature after the addition is finished, filtering to obtain a crystallized product, drying the obtained crystallized product at low temperature, and preparing to obtain the ammonium dihydrogen phosphate compound. According to the invention, ammonium dihydrogen phosphate and organic sugar can be mixed on the molecular scale, and the method has the characteristic that the phase distribution is uniform, so that a phenomenon that the carbon cladding is non-uniform due to non-uniform mixing of a carbon source in the process of synthesizing lithium iron phosphate in an organic solvent system by taking ammonium dihydrogen phosphate as a raw material.

Description

technical field [0001] The invention relates to a preparation process for synthesizing lithium iron phosphate raw materials for lithium battery cathode material, in particular to a synthesis method of ammonium dihydrogen phosphate compound, Background technique [0002] Lithium iron phosphate material is recognized as the safest lithium-ion battery cathode material, and is widely used in energy storage equipment, power tools, automotive power batteries, mobile power supplies, etc. Due to the poor ion conductivity of the lithium iron phosphate material itself, the deintercalation speed of lithium ions is not ideal during the charging and discharging process, which affects its electrochemical performance. At present, it is mainly electrochemically modified by carbon coating, doping and other methods. sex. In the electrochemical performance of carbon-coated modified lithium iron phosphate materials, the preferred carbon source is organic sugars, especially sucrose and glucose,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58
CPCC01B25/28H01M4/5825Y02E60/10
Inventor 刘大军吴以洪
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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